scholarly journals An automated platform for in situ serial crystallography at room temperature

IUCrJ ◽  
2020 ◽  
Vol 7 (6) ◽  
pp. 1009-1018
Author(s):  
Zhong Ren ◽  
Cong Wang ◽  
Heewhan Shin ◽  
Sepalika Bandara ◽  
Indika Kumarapperuma ◽  
...  
Keyword(s):  
Data Collection ◽  
Room Temperature ◽  
Protein Structures ◽  
Routine Data ◽  
Protein Crystals ◽  
X Ray Diffraction ◽  
X Ray ◽  
Serial Crystallography ◽  
Routine Data Collection

Direct observation of functional motions in protein structures is highly desirable for understanding how these nanomachineries of life operate at the molecular level. Because cryogenic temperatures are non-physiological and may prohibit or even alter protein structural dynamics, it is necessary to develop robust X-ray diffraction methods that enable routine data collection at room temperature. We recently reported a crystal-on-crystal device to facilitate in situ diffraction of protein crystals at room temperature devoid of any sample manipulation. Here an automated serial crystallography platform based on this crystal-on-crystal technology is presented. A hardware and software prototype has been implemented, and protocols have been established that allow users to image, recognize and rank hundreds to thousands of protein crystals grown on a chip in optical scanning mode prior to serial introduction of these crystals to an X-ray beam in a programmable and high-throughput manner. This platform has been tested extensively using fragile protein crystals. We demonstrate that with affordable sample consumption, this in situ serial crystallography technology could give rise to room-temperature protein structures of higher resolution and superior map quality for those protein crystals that encounter difficulties during freezing. This serial data collection platform is compatible with both monochromatic oscillation and Laue methods for X-ray diffraction and presents a widely applicable approach for static and dynamic crystallographic studies at room temperature.

scholarly journals High-throughput in situ X-ray screening of and data collection from protein crystals at room temperature and under cryogenic conditions

2018 ◽  
Vol 13 (2) ◽  
pp. 260-292 ◽  
Author(s):  
Jana Broecker ◽  
Takefumi Morizumi ◽  
Wei-Lin Ou ◽  
Viviane Klingel ◽  
Anling Kuo ◽  
...  
Keyword(s):  
Data Collection ◽  
High Throughput ◽  
Room Temperature ◽  
Protein Crystals ◽  
X Ray ◽  
Cryogenic Conditions

Photoluminescence Enhancement of CdS Nanocrystals Fabricated on Dithiocarbamate Functionalized PET Substrates

2012 ◽  
Vol 512-515 ◽  
pp. 1511-1515
Author(s):  
Chun Lin Zhao ◽  
Li Xing ◽  
Xiao Hong Liang ◽  
Jun Hui Xiang ◽  
Fu Shi Zhang ◽  
...  
Keyword(s):  
Room Temperature ◽  
Hexagonal Structure ◽  
Diffraction Measurement ◽  
X Ray Diffraction ◽  
Visible Absorption ◽  
X Ray ◽  
Cds Nanocrystals ◽  
Morphological Studies ◽  
Transmission Electron

Cadmium sulfide (CdS) nanocrystals (NCs) were self-assembled and in-situ immobilized on the dithiocarbamate (DTCs)-functionalized polyethylene glycol terephthalate (PET) substrates between the organic (carbon disulfide diffused in n-hexane) –aqueous (ethylenediamine and Cd2+ dissolved in water) interface at room temperature. Powder X-ray diffraction measurement revealed the hexagonal structure of CdS nanocrystals. Morphological studies performed by scanning electron microscopy (SEM) and high-resolution transmission electron microscope (HRTEM) showed the island-like structure of CdS nanocrystals on PET substrates, as well as energy-dispersive X-ray spectroscopy (EDS) confirmed the stoichiometries of CdS nanocrystals. The optical properties of DTCs modified CdS nanocrystals were thoroughly investigated by ultraviolet-visible absorption spectroscopy (UV-vis) and fluorescence spectroscopy. The as-prepared DTCs present intrinsic hydrophobicity and strong affinity for CdS nanocrystals.

In Situ Synchrotron X-Ray Diffraction Study of a Deformed Cu-Fe-P Alloy during Heating

2016 ◽  
Vol 850 ◽  
pp. 191-196 ◽  
Author(s):  
Wei Wang ◽  
Cun Lei Zou ◽  
Ren Geng Li ◽  
Wen Wen ◽  
Hui Jun Kang ◽  
...  
Keyword(s):  
Room Temperature ◽  
Lattice Distortion ◽  
Copper Matrix ◽  
Heating Process ◽  
Recrystallization Process ◽  
Full Width ◽  
X Ray Diffraction ◽  
Dramatic Decrease ◽  
X Ray

In situ synchrotron X-ray diffraction was used to study a deformed Cu-0.88 Fe-0.24 P alloy during heating process. The measurements were performed at room temperature and also at high temperatures up to 893 K in order to determine the recovery, ageing and recrystallization process. With the increase of temperature, the angles of copper matrix peaks moved left and the FWHM (full width at half maximum) decreased slightly. Fe3P precipitates were first detected at 533 K, reached the maximum at 673 K, and re-dissolved into matrix at 853 K. A dramatic decrease in FWHM was observed accompanied by the precipitation of Fe3P phases, indicating the reduction of lattice distortion of copper matrix.

scholarly journals Insertion of Phosphenium Ions into a Bicyclo[1.1.0]Tetraphosphabutane Iron Complex

Molecules ◽  
2021 ◽  
Vol 26 (13) ◽  
pp. 3920
Author(s):  
Martin Weber ◽  
Gábor Balázs ◽  
Alexander V. Virovets ◽  
Eugenia Peresypkina ◽  
Manfred Scheer
Keyword(s):  
Diffraction Analysis ◽  
Room Temperature ◽  
31P Nmr ◽  
Spectroscopic Studies ◽  
Iron Complex ◽  
The Novel ◽  
X Ray Diffraction ◽  
X Ray ◽  
Phosphenium Ions

By reacting [{Cp‴Fe(CO)2}2(µ,η1:1-P4)] (1) with in situ generated phosphenium ions [Ph2P][A] ([A]− = [OTf]− = [O3SCF3]−, [PF6]−), a mixture of two main products of the composition [{Cp‴Fe(CO)2}2(µ,η1:1-P5(C6H5)2)][PF6] (2a and 3a) could be identified by extensive 31P NMR spectroscopic studies at 193 K. Compound 3a was also characterized by X-ray diffraction analysis, showing the rarely observed bicyclo[2.1.0]pentaphosphapentane unit. At room temperature, the novel compound [{Cp‴Fe}(µ,η4:1-P5Ph2){Cp‴(CO)2Fe}][PF6] (4) is formed by decarbonylation. Reacting 1 with in situ generated diphenyl arsenium ions gives short-lived intermediates at 193 K which disproportionate at room temperature into tetraphenyldiarsine and [{Cp‴Fe(CO)2}4(µ4,η1:1:1:1-P8)][OTf]2 (5) containing a tetracyclo[3.3.0.02,7.03,6]octaphosphaoctane ligand.

In situ high temperature X-ray diffraction study of the kinetics of phase separation in the uranium-plutonium mixed oxide (U0.55Pu0.45)O2-x

2014 ◽  
Vol 1645 ◽  
Author(s):  
Romain VAUCHY ◽  
Renaud.C. BELIN ◽  
Anne-Charlotte ROBISSON ◽  
Fiqiri HODAJ
Keyword(s):  
Phase Separation ◽  
Room Temperature ◽  
Mixed Oxides ◽  
Oxygen Stoichiometry ◽  
X Ray Diffraction ◽  
Fundamental Interest ◽  
X Ray ◽  
Uranium Plutonium ◽  
Kinetics Of

ABSTRACTUranium-plutonium mixed oxides incorporating high amounts of plutonium are considered for future nuclear reactors. For plutonium content higher than 20%, a phase separation occurs, depending on the temperature and on the oxygen stoichiometry. This phase separation phenomenon is still not precisely described, especially at high plutonium content. Here, using an original in situ fast X-ray diffraction device dedicated to radioactive materials, we evidenced a phase separation occurring during rapid cooling from 1773 K to room temperature at the rate of 0.05 and 2 K per second for a (U0.55Pu0.45)O2-x compound under a reducing atmosphere. The results show that the cooling rate does not impact the lattice parameters of the obtained phases at room temperature but their fraction. In addition to their obvious fundamental interest, these results are of utmost importance in the prospect of using uranium-plutonium mixed oxides with high plutonium content as nuclear fuels.

IN SITU SYNTHESIS, CHARACTERIZATION AND FREQUENCY DEPENDENT AC CONDUCTIVITY OF POLYANILINE/CoFe2O4 NANOCOMPOSITES

2011 ◽  
Vol 01 (03) ◽  
pp. 357-362 ◽  
Author(s):  
G. D. PRASANNA ◽  
H. S. JAYANNA
Keyword(s):  
Ac Conductivity ◽  
Room Temperature ◽  
In Situ Polymerization ◽  
In Situ Synthesis ◽  
Electron Micrograph ◽  
Frequency Range ◽  
X Ray Diffraction ◽  
Scanning Electron Micrograph ◽  
X Ray

The polyaniline (PANI)/ CoFe2O4 nanocomposites were prepared by an In Situ polymerization of aniline in an aqueous solution. The composites were characterized by X-ray diffraction (XRD), Fourier transform infrared (FTIR) spectrum,thermogravimetric analysis (TGA) and scanning electron micrograph (SEM). The AC conductivity and dielectric properties of these composites were investigated in the frequency range 1 kHz–10 MHz at room temperature. The AC conductivity was found to be constant up to 1 MHz and thereafter it increases steeply and it was observed maximum for the PANI with 60 wt% of CoFe2O4 nanocomposite. At lower frequencies the values of dielectric constant is maximum for pure CoFe2O4 nanoparticles.

Green Synthesis of Semi-IPN Hydrogel-Silver Nanocomposites by a Biotemplate Redox Technique at Room Temperature

2012 ◽  
Vol 468-471 ◽  
pp. 1974-1977
Author(s):  
Wen Wu ◽  
Dong Sheng Wang
Keyword(s):  
Silver Nanoparticles ◽  
Green Synthesis ◽  
Silver Nitrate ◽  
Room Temperature ◽  
In Situ Reduction ◽  
X Ray Diffraction ◽  
Silk Sericin ◽  
X Ray ◽  
Silver Nanocomposites

Semi-IPN hydrogels in which silk sericin (SS) chains were physically dispersed throughout dextran (Dex) gel networks were synthesized. Highly stable distributed silver nanoparticles have been prepared using these semi-IPN hydrogels as a carrier via in situ reduction of silver nitrate without the addition of any reducing agent. The resultant semi-IPN hydrogel-silver nanocomposites were characterized by X-ray diffraction (XRD). And the swelling behavior of the hydrogles was also studied.

scholarly journals Lactide polymerization with iron alkoxide complexes

2015 ◽  
Vol 93 (6) ◽  
pp. 594-601 ◽  
Author(s):  
Arek Keuchguerian ◽  
Berline Mougang-Soume ◽  
Frank Schaper ◽  
Davit Zargarian
Keyword(s):  
Single Crystal ◽  
Room Temperature ◽  
Side Reactions ◽  
X Ray Diffraction ◽  
Iron Cluster ◽  
X Ray ◽  
H Nmr ◽  
Exchange Product

This report presents the results of a study on the preparation of iron alkoxide complexes chelated by diiminopyridine ligands and their role in the room temperature polymerization of rac-lactide. Reaction of N,N′-(p-R-C6H4CH2)2-diiminopyridines (R = H (1), F (2)) with FeX2 (X = Cl, Br) yielded the homoleptic complexes [(1)2Fe][FeX4] or [(2)2Fe][FeX4], respectively. Treating the latter with Na[BPh4] afforded the anion exchange product [(2)2Fe][BPh4]2, which was characterized by 1H NMR and absorption spectroscopy, combustion analysis, and single crystal X-ray diffraction. Various attempts to grow crystals of [(1)2Fe][FeX4] and [(2)2Fe][FeX4] culminated in the isolation of single crystals of [(2)2Fe][Cl6Fe2O] that was characterized by X-ray diffraction. Attempted synthesis of well-defined, mononuclear alkoxide derivatives from [(1)2Fe]2+ or [(2)2Fe]2+ gave mostly intractable products, but in one case we obtained the crystallographically characterized sodium iron cluster Na4Fe2(OC6H4F)8(THF)2. An aryloxide derivative proved accessible by reaction of NaOC6H4F with the mono-ligand precursor LFeCl2 (L = N,N′-dimesityl-diiminopyridine), but characterization of LFe(OC6H4F)2 was limited to a single crystal X-ray diffraction analysis, owing to unsuccessful attempts at isolating pure samples. The difficulties encountered in the isolation of pure alkoxide derivatives prompted us to use in-situ generated LFe(OEt)2 for studying the polymerization of rac-lactide. This system was found to be moderately active at room temperature and with a slight preference for the formation of a heterotactic polymer (Pr = 0.54–0.65). Large polydispersities of 1.5–2.0 indicated the presence of transesterification side-reactions, which were confirmed by the presence of peaks with m/z = n 144 + M(EtOH) + M(Na+) and m/z = (n + 0.5) 144 + M(EtOH) + M(Na+) in MALDI-MS.

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